Carbohydrate chains released by trifluoroacetolysis of whole tissues, tissued fractions, or cells grown in culture, are easily recovered in nearly quantitative yield and reconstitued to their native form. Analysis of the majority of oligosaccharides containing six or fewer monosaccharide units is performed by combined gas chromoatography and mass spectrometry of permethylated, N-trifluuoroacetylated oligosaccharide derivatives. Analysis for certain specific oligosaccharides is carried out by radioimmunosassary using antibodies produced against purified oligosaccharides coupled to polypeptide carriers. It is anticipated that the repertoire of oligosaccharide chains produced by cells or tissues will reflect states of cellular differentiation and reveal potential cell surface markers.